CN113621336B - High-temperature curing silane modified polyether sealant and preparation method and use method thereof - Google Patents

High-temperature curing silane modified polyether sealant and preparation method and use method thereof Download PDF

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CN113621336B
CN113621336B CN202110860241.3A CN202110860241A CN113621336B CN 113621336 B CN113621336 B CN 113621336B CN 202110860241 A CN202110860241 A CN 202110860241A CN 113621336 B CN113621336 B CN 113621336B
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modified polyether
silane modified
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sealant
polyether sealant
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CN113621336A (en
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刘伟明
陈军
沈峰
柴梦洒
裘杭建
何永富
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Hangzhou Zhijiang Silicone Chemicals Co Ltd
Hangzhou Zhijiang New Material Co Ltd
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Hangzhou Zhijiang Silicone Chemicals Co Ltd
Hangzhou Zhijiang New Material Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J171/00Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

The application relates to the field of sealants, in particular to a high-temperature curing silane modified polyether sealant and a preparation method and a use method thereof.

Description

High-temperature curing silane modified polyether sealant and preparation method and use method thereof
Technical Field
The application relates to the field of sealants, in particular to a high-temperature cured silane modified polyether sealant as well as a preparation method and a use method thereof.
Background
The sealant is a chemical raw material commonly used in the fields of vehicles, ships, electromechanics and buildings, is commonly used for bonding and sealing mechanical structures, and needs to have the physical and chemical properties of dust prevention, water prevention, earthquake resistance, tear resistance and the like.
In part of the mechanical equipment treatment process, electrophoretic coating is needed, and in the process, the whole mechanical structure needs to be immersed in treatment liquid for treatment. In the above process, the sealant is generally heated to 150-200 ℃ for several hours or even tens of hours, and bubbles are easily generated in the sealant, thereby affecting the quality of the sealant.
Disclosure of Invention
In order to reduce bubbles generated by electrophoresis treatment of products in the sealant, the application provides a high-temperature curing silane modified polyether sealant, and a preparation method and a use method thereof
Firstly, the application provides a high-temperature curing silane modified polyether sealant which comprises the following components in parts by mass:
Figure GDA0003504238240000011
wherein, the silane modified polyether is any one of SAX350, SAX400, SAX750 or SAX440 of kaneka company, and the plasticizer can select one or more of phthalate compounds and polyether polyols. The phthalate ester compound is diisononyl phthalate, diisooctyl phthalate and diisodecyl phthalate. The polyether polyol is PPG1000, PPG2000, PPG3000, PPG4000 or PPG 8000.
The thixotropic agent can be any one of polyamide wax, hydrogenated castor oil and fumed silica.
In the technical scheme, the silane modified polyether is used as a main body, and the epoxy silane coupling agent and the organic tin curing agent are used as auxiliary materials, so that the sealant can be cured at high temperature and has a good high-temperature resistant effect.
Epoxy ring-opening reaction can occur between the epoxy silane coupling agent and the organic tin curing agent, and the formed tin-oxygen bond has higher bond energy and higher reaction rate, so that the sealant can be rapidly cured in the heating process, the phenomenon that the sealant generates bubbles in the electrophoresis process is reduced, and the quality of the sealant is greatly improved.
The stabilizer comprises the following components:
0.1-3 parts of an ultraviolet absorbent;
0.1-3 parts of hindered amine light stabilizer;
4-10 parts of hindered phenol stabilizers or phosphite ester heat stabilizers.
Wherein the hindered phenol heat stabilizer can be antioxidant 1076 or antioxidant 245,
in the technical scheme, the combination of the ultraviolet absorber, the light stabilizer and the heat stabilizer enables the sealant to keep stable performance in the heating curing process and the electrophoresis process, and improves the strength of the sealant.
Optionally, the ceramic material further comprises 0.1-0.4 parts by mass of liquid ceramic.
The liquid ceramic has stronger reactivity and crosslinking property, and can quickly react with an organic tin curing agent and an epoxy silane coupling agent in a system to form a network crosslinking structure in the high-temperature curing process, so that the whole structure of the sealant is more stable after the sealant is cured at high temperature, and bubbles are not easily generated in the electrophoresis process.
Optionally, the filler contains no more than 2% of nano silicon nitride by total mass of the filler.
In the preparation process, the silicon-nitrogen bond on the surface of the nano silicon nitride can react with the epoxy group on the epoxy silane coupling agent to form a silicon-oxygen bond, the bond energy of the silicon-oxygen bond is strong, and a stable coupling structure can be formed, so that the nano silicon nitride can be used as an intersection point of a network structure in a system to form a more stable structure, and the possibility of generating bubbles in the electrophoresis treatment process after the sealant is cured at high temperature is further reduced.
Optionally, the filler is a combination of at least one of nano calcium carbonate, ground calcium carbonate, clay, talcum powder and organic bentonite and nano silicon nitride.
The filler and the nano silicon nitride are selected to be combined, and the formed adhesive layer has good strength and toughness and good performance.
Optionally, the filler is a combination of nano calcium carbonate, ground limestone and nano silicon nitride, and the mass ratio of the nano calcium carbonate to the ground limestone to the nano silicon nitride is (45-60) to (25-40) to 1.
The combination is selected as the filler, the sealant can keep better fluidity and stronger stability in the curing process, and the mechanical property is better after curing, so that the sealant has better strength while being not easy to generate bubbles in the electrophoresis process.
Optionally, the paint also comprises 0.1-0.2 parts by mass of polyamine curing agent.
Wherein the polyamine curing agent can be any one of m-phenylenediamine, m-xylylenediamine and benzidine.
In the technical scheme, the amino in the polyamine curing agent has better reactivity, and the crosslinking degree in the sealant can be improved through the multi-reactivity; meanwhile, the polyamine curing agent generally has a flexible molecular chain structure, so that a better macromolecular winding structure can be formed in a system, the influence on the flowability of the sealant before curing is small, and the thermal stability and the strength of the cured sealant are improved to a certain extent.
Optionally, the coating also comprises 1.0-1.4 parts by mass of bisphenol A.
The bisphenol A dihydric phenol hydroxyl structure and the relatively rigid benzene ring structure can play a role in shaping the whole structure of the sealant in the curing process of the sealant, so that the molecular chain inside the sealant is not easy to move in the heating process, the morphological change in the heating process of the sealant is reduced, and the thermal stability of the sealant is further improved.
Meanwhile, the application also relates to a preparation method of the high-temperature curing silane modified polyether sealant, which is used for preparing the high-temperature curing silane modified polyether sealant and comprises the following specific steps:
s1, mixing the components except the epoxy silane coupling agent and the organic tin curing agent, and stirring at 800-1500 rpm for 40-80 min to obtain a first mixed component;
s2, heating the first mixed component to 100-130 ℃, and continuously stirring at 800-1500 rpm until the first mixed component is dehydrated to obtain a second mixed component;
s3, cooling the second mixed component to 40-50 ℃, adding an epoxy silane coupling agent, and stirring at 200-300 rpm for 15-30 min to obtain a third mixed component;
s4, adding an organic tin curing agent into the third mixed component, continuously keeping the temperature at 40-50 ℃, stirring at 200-300 rpm for 15-30 min, and then discharging after vacuum dispersion to obtain the high-temperature cured silane modified polyether sealant; during the above stirring, vacuum was maintained.
In the preparation scheme, the components are fully mixed and then dehydrated by rapid stirring, so that the hydrolysis reaction of the silane coupling agent and the curing agent is reduced, and the subsequent bubbles generated by water evaporation in the heating process are reduced after moisture is removed. After the dehydration is finished, the silane coupling agent and the organic tin curing agent are added in sequence under the condition of slow stirring, one end of silane of the silane coupling agent is adsorbed on the edge of the filler, and the organic tin curing agent is added.
In addition, the application also relates to a using method of the high-temperature curing silane modified polyether sealant, the high-temperature curing silane modified polyether sealant is cured for 40-60 hours at the temperature of 97-103 ℃, then cured for 30-60 min at the temperature of 118-122 ℃, then cured for 10-20 min at the temperature of 145-155 ℃, and finally cured for 8-12 min at the temperature of 175-190 ℃.
In the process, the silane coupling agent is firstly reacted with the organic tin curing agent with stronger activity to form a primary curing effect, and then is further reacted with other components to strengthen the curing effect, so that the finally formed sealing colloid system has better performance, and meanwhile, in the subsequent electrophoresis treatment, fewer bubbles are generated, and the sealing colloid system has better property.
In summary, the present application includes at least one of the following advantages:
1. in the application, the combination of the organic tin curing agent and the epoxy silane coupling agent is adopted, so that the sealant has better heat resistance, the generation of bubbles is reduced in electrophoresis treatment, and the performance of the sealant is improved.
2. In the further setting of this application, through adding liquid pottery, further improve the inside degree of crosslinking of sealed glue, reduce its bubble that produces in the electrophoresis process.
3. In the further setting of the application, the overall physical property of the sealant is further improved by adding the nano silicon nitride into the filler.
Detailed Description
The present application will be described in further detail with reference to examples.
In the following examples, the sources of some of the feedstocks are shown in table 1.
TABLE 1 table of sources of materials
Silane modified polyether The various silane-modified polyethers were purchased from kaneka corporation
PPG1000 Basff PEG1000
Benzotriazole ultraviolet absorbers TINUVIN 326
Liquid ceramics Alpha, MW1400
Hindered amine light stabilizers Light stabilizer 292
Hindered phenol antioxidants Pasteur antioxidant 1076
Phosphite heat stabilizer Irgafos168
Polyamine curing agents Biphenylamine
Nano calcium carbonate The plant type of the Baishi industrial plant can be 50-100 nm
Ground calcium carbonate The plant type of the Baishi industrial plant is 10-20 μm
Clay clay 1-50 mu m of first-grade powdery clay of lingshou mica ore
Talcum powder Lu mineral, 10-50 μm
Organic bentonite Anji Tianlong, BT-838D
Nano silicon nitride Cloud magnesium technology of 50-200 nm
Examples 1 to 5, the raw materials used for the high temperature curing of the silane modified polyether sealants are shown in table 2.
Table 2 selection of Components (g) in examples 1 to 5
Components Example 1 Example 2 Example 3 Example 4 Example 5
Silane modified polyether 80 90 100 110 120
Plasticizer 40 45 50 55 60
Thixotropic agent 10 5 2 1 0.5
Filler material 250 225 200 175 150
Ultraviolet absorber 1 1 1 1 1
Hindered amine light stabilizers 1 1 1 1 1
Hindered phenol antioxidants 6 6 6 6 6
Epoxy silane coupling agent 1.5 1.5 1.5 1.5 1.5
Organotin curing agents 1 1 1 1 1
Wherein, the filler is a compound system formed by organic bentonite and nano calcium carbonate in a mass ratio of 1: 1, the plasticizer is a compound system formed by diisononyl phthalate and PPG1000 in a mass ratio of 0.3: 1, and the thixotropic agent is polyamide wax. The ultraviolet absorbent is benzotriazole ultraviolet absorbent. The epoxy silane coupling agent is 2- (3, 4-epoxy cyclohexyl) ethyl trimethoxy silane, and the organic tin curing agent is dimethyl tin oxide.
In embodiments 1 to 5, the preparation method of the high-temperature cured silane modified polyether sealant comprises the following steps:
s1, mixing the silane modified polyether, the plasticizer, the thixotropic agent, the filler and the stabilizer and stirring at 1000rpm for 60min to obtain a first mixed component;
s2, heating the first mixed component to 110 ℃, and continuing stirring at 1000rpm for 120min to dehydrate the system to obtain a second mixed component;
s3, cooling the second mixed component to 45 ℃, adding an epoxy silane coupling agent, and stirring at 150rpm for 25min to obtain a third mixed component;
s4, adding an organic tin curing agent into the third mixed component, stirring at 250rpm for 25min, and discharging after vacuum dispersion to obtain the high-temperature cured silane modified polyether sealant;
the stirring process is controlled to be under the air pressure of 10-1And (4) under the condition of Pa.
Examples 6 to 12, the difference between the high temperature curing silane modified polyether sealant and example 2 is that the stabilizer is adjusted, specifically as shown in table 3.
Table 3, examples 6-12 stabilizer selection and dosage
Figure GDA0003504238240000051
Examples 13 to 27, the difference between the high temperature curing silane modified polyether sealant and example 3 is that in step S1, liquid ceramic is additionally added, and the components of the filler are adjusted, as shown in table 4.
Table 4, examples 13 to 27 partial parameters of the amount of materials added (g)
Figure GDA0003504238240000052
Figure GDA0003504238240000061
Example 28, a high temperature cure silane modified polyether sealant, the same as example 3 except that in step S1, 0.1g of a polyamine curative was also added.
Example 29, a high temperature cure silane modified polyether sealant, the same as that of example 3, was prepared by also adding 0.2g of polyamine curative in step S1.
Example 30, a high temperature cure silane modified polyether sealant, the same as example 3 except that in step S1, 0.3g of polyamine curative was also added.
Example 31, a high temperature cure silane modified polyether sealant, the same as that of example 3, was prepared by also adding 1.0g of bisphenol a in step S1.
Example 32, a high temperature cure silane modified polyether sealant, the same as that of example 3, was prepared by also adding 1.4g of bisphenol a in step S1.
Example 33 a high temperature cure silane modified polyether sealant was prepared in accordance with the teachings of example 3 by also adding 2.0g of bisphenol a in step S1.
Example 34 a high temperature cure silane modified polyether sealant differs from example 23 in that in step S1, 0.2g of a polyamine curative and 1.4g of bisphenol a are also added.
Example 35, a high temperature cure silane modified polyether sealant, different from example 23, in that the stirring time of step S1 is 40min, the stirring rate is 800rpm, the temperature of step S2 is 100 ℃, the stirring rate is 800rpm, the stirring time of step S3 is 15min, the stirring temperature is 40 ℃, the stirring rate is 200rpm, the stirring time of step S4 is 15min, the stirring temperature is 40 ℃, and the stirring rate is 200 rpm.
Example 36, a high temperature cure silane modified polyether sealant, different from example 23, in that the stirring time of step S1 is 80min, the stirring rate is 1500rpm, the temperature of step S2 is 130 ℃, the stirring rate is 1500rpm, the stirring time of step S3 is 30min, the stirring temperature is 50 ℃, the stirring rate is 300rpm, the stirring time of step S4 is 30min, the stirring temperature is 50 ℃, and the stirring rate is 300 rpm.
In examples 37 to 38, the difference between the high temperature curing silane modified polyether sealant and example 3 is that the selection of the epoxy silane modified coupling agent and the organotin curing agent is shown in table 5.
Table 5, selection of silane coupling agent and curing agent in examples 37 to 38
Figure GDA0003504238240000071
For the above examples, comparative examples were set as follows:
comparative examples 1 to 6, a silane-modified polyether sealant, which is different from example 3 in that different silane coupling agents and curing agents are selected, and is specifically shown in table 6.
Selection of silane coupling agent and curing agent in Table 6 and comparative examples 1-6
Figure GDA0003504238240000072
For the above examples and comparative examples, the following procedure was carried out, which were prepared as samples:
the sealant prepared in the above examples and comparative examples is injected into a model, cured at 100 ℃ for 45h, cured at 120 ℃ for 40min, cured at 150 ℃ for 15min, and cured at 180 ℃ for 10min to obtain experimental samples 1-38 and comparative samples 1-6.
The percentage tensile strength, the maximum tensile strength and the elongation at break of the sample after two different heat treatment conditions are measured according to GB/T528-2009 determination of tensile stress strain performance of vulcanized rubber or thermoplastic rubber. And simultaneously, whether bubbles exist in the sealant is observed by naked eyes.
Heat treatment conditions A: treated at 150 ℃ for 15min and then left at 23 ℃ for 3 d.
Heat treatment conditions B: treating at 150 deg.C for 30min, treating at 180 deg.C for 30min, and standing at 23 deg.C for 3 d.
First, the properties of the experimental samples and the comparative samples prepared in examples 1 to 5, examples 37 to 38, and comparative examples 1 to 6 were measured and shown in Table 7.
TABLE 7 Experimental results for Experimental samples 1-5, Experimental samples 37-38, and control samples 1-6
Figure GDA0003504238240000073
Figure GDA0003504238240000081
According to the experimental data, the combination of the epoxy silane coupling agent and the organic tin curing agent is adopted, so that the sealant can still keep better strength and elasticity after being subjected to high-temperature treatment for a longer time, and bubbles can not be generated, so that the sealant is not easy to deteriorate due to high temperature of an electrophoresis environment in the electrophoresis process and has stronger high-temperature resistance.
The epoxy silane coupling agent and the organic tin curing agent can form various reaction types including a chelation reaction of oxygen and tin, a bonding formation of a tin-oxygen bond and the like, and the reaction can be rapidly carried out at a high temperature, so that the sealant can be completely cured. As can be seen by comparison with comparative examples 1 to 6, only the epoxypropane silane coupling agent and the organotin curing agent can achieve the above-described effects.
Further, the results of experiments on the sealant samples of examples 6 to 12 are shown in table 8.
TABLE 8 Experimental results of Experimental samples 6-12
Figure GDA0003504238240000082
The stabilizer is adjusted in the embodiment, and since the experimental sample is prepared in a high-temperature curing manner in the application, the stabilizer needs to be added to reduce the influence on the sealant in the high-temperature curing process. According to the experiments, the sealant can keep good mechanical properties during curing through the combination of the ultraviolet absorber, the hindered amine light stabilizer and the heat stabilizer.
Further, the results of experiments performed on the experimental samples 13 to 27 are shown in table 9.
TABLE 9 Experimental results of Experimental samples 13 to 27
Figure GDA0003504238240000091
In the embodiment, the liquid ceramic is further added, the liquid ceramic has strong coupling capacity, and has good reaction performance with silane coupling agent, silane modified resin and the like in a system, the formed cross-linked structure can obviously improve the mechanical performance of the sealant, and simultaneously, the loss of the mechanical performance of the sealant after heat treatment is reduced. However, when the liquid ceramic is excessively added, the elasticity of the sealant is deteriorated, and meanwhile, in the above embodiment, the filler is adjusted, and experiments show that after the nano silicon nitride is added into the filler, the silicon nitrogen bond on the surface can react with the epoxy group on the epoxy silane coupling agent to form a silicon oxygen bond, so that the structure formed in the sealant is more stable, and the high temperature resistance of the sealant is better.
In addition, in embodiments 21-23, the combination of nano calcium carbonate and ground calcium carbonate is selected, both calcium carbonates do not participate in the reaction of the system, the coupling structure formed by silicon nitride and liquid ceramic is not damaged, the formed composite system has good processability, and the air in the thermosetting process can be rapidly discharged, so that the overall elasticity and mechanical strength are improved.
Further, the results of experiments performed on the experimental samples 28 to 36 are shown in table 10.
TABLE 10 Experimental results of Experimental samples 28-36
Figure GDA0003504238240000092
Figure GDA0003504238240000101
In embodiments 28 to 30, a polyamine curing agent is further added, which improves the degree of crosslinking in the system, so that the sealant has less mechanical strength and elastic loss after high temperature treatment. In the embodiments 31-33, the bisphenol A is added, and the thermal stability of the sealant is further improved by the binary reaction effect of the bisphenol A, so that the maximum tensile strength is better improved.
Additionally, the curing process of the sealant was adjusted based on the sealant prepared in example 3 to provide the following examples.
Example 39, method of using a high temperature cured silane modified polyether sealant, the high temperature cured silane modified polyether sealant prepared in example 3 was cured at 97 ℃ for 60h, then at 118 ℃ for 60min, then at 145 ℃ for 20min, and finally at 175 ℃ for 12min to obtain an experimental sample 39.
Example 40, method of using a high temperature cured silane modified polyether sealant, the high temperature cured silane modified polyether sealant prepared in example 3 was cured at 103 ℃ for 40h, then at 122 ℃ for 30min, then at 155 ℃ for 10min, and finally at 175 ℃ for 12min to obtain an experimental sample 40.
Example 41, method of use of high temperature cured silane modified polyether sealant the high temperature cured silane modified polyether sealant prepared in example 3 was first cured at 100 ℃ for 48h and then at 120 ℃ for 90min to obtain test sample 41.
Example 42, method of using a high temperature cured silane modified polyether sealant the high temperature cured silane modified polyether sealant prepared in example 3 was first cured at 100 ℃ for 75 hours to obtain test sample 42.
Example 43, method of using a high temperature cured silane modified polyether sealant, the high temperature cured silane modified polyether sealant prepared in example 3 was first cured at 140 ℃ for 240min to obtain an experimental sample 43.
The examples 39-43 all can achieve complete curing of the sealant, and the property measurements are shown in Table 11.
TABLE 11 Experimental results of Experimental samples 28-36
Figure GDA0003504238240000111
According to the experimental data, after the heating and curing are carried out by adopting the method, in order to realize a better curing effect, bubbles are basically not generated after the heat treatment, and the strength loss is small.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims (7)

1. The high-temperature curing silane modified polyether sealant is characterized by comprising the following components in parts by mass:
80-120 parts of silane modified polyether;
40-60 parts of a plasticizer;
0.5-10 parts of a thixotropic agent;
150-250 parts of a filler;
4.2-16 parts of a stabilizer;
1-2 parts of epoxy silane coupling agent;
0.5-1.5 parts of organic tin curing agent;
1.0-1.4 parts of bisphenol A;
0.1-0.4 parts of liquid ceramic;
the filler contains no more than 2 percent of nano silicon nitride by the total mass of the filler.
2. The high temperature cure silane modified polyether sealant of claim 1, wherein the stabilizer comprises the following components:
0.1-3 parts of an ultraviolet absorbent;
0.1-3 parts of hindered amine light stabilizer;
4-10 parts of hindered phenol stabilizers or phosphite ester heat stabilizers.
3. The high temperature curing silane modified polyether sealant as claimed in claim 1, wherein the filler is a combination of at least one of nano calcium carbonate, heavy calcium carbonate, clay, talc and organic bentonite and nano silicon nitride.
4. The high-temperature curing silane modified polyether sealant as claimed in claim 3, wherein the filler is a combination of nano calcium carbonate, heavy calcium carbonate and nano silicon nitride, and the mass ratio of the nano calcium carbonate to the heavy calcium carbonate to the nano silicon nitride is (45-60) to (25-40) to 1.
5. The high-temperature curing silane modified polyether sealant as claimed in claim 1, further comprising 0.1-0.2 parts by mass of polyamine curing agent.
6. The preparation method of the high-temperature curing silane modified polyether sealant is characterized by being used for preparing the high-temperature curing silane modified polyether sealant as claimed in any one of claims 1 to 5, and comprising the following specific steps:
s1, mixing the components except the epoxy silane coupling agent and the organic tin curing agent, and stirring at 800-1500 rpm for 40-80 min to obtain a first mixed component;
s2, heating the first mixed component to 100-130 ℃, and continuously stirring at 800-1500 rpm until the first mixed component is dehydrated to obtain a second mixed component;
s3, cooling the second mixed component to 40-50 ℃, adding an epoxy silane coupling agent, and stirring at 200-300 rpm for 15-30 min to obtain a third mixed component;
s4, adding an organic tin curing agent into the third mixed component, continuously keeping the temperature at 40-50 ℃, stirring at 200-300 rpm for 15-30 min, and then discharging after vacuum dispersion to obtain the high-temperature cured silane modified polyether sealant;
during the above stirring, vacuum was maintained.
7. The use method of the high temperature curing silane modified polyether sealant as claimed in any one of claims 1 to 5 or the high temperature curing silane modified polyether sealant as claimed in claim 6, wherein the high temperature curing silane modified polyether sealant is cured at 97 to 103 ℃ for 40 to 60 hours, then cured at 118 to 122 ℃ for 30 to 60min, then cured at 145 to 155 ℃ for 10 to 20min, and finally cured at 175 to 190 ℃ for 8 to 12 min.
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Publication number Priority date Publication date Assignee Title
CN102504258A (en) * 2011-10-12 2012-06-20 中国人民解放军国防科学技术大学 Method for preparing high-temperature resisting organic adhesive by utilizing liquid silicon carbide precursor
CN108047970A (en) * 2017-12-12 2018-05-18 苏州铂邦胶业有限公司 A kind of good silicone sealant of weatherability and preparation method thereof
CN109401710A (en) * 2018-09-30 2019-03-01 广州市白云化工实业有限公司 Dual-component silicane modified polyether seal glue and preparation method thereof
CN111394034B (en) * 2020-05-21 2021-08-24 广州市白云化工实业有限公司 Single-component silane modified polyether sealant for prefabricated building and preparation method thereof
CN111635633B (en) * 2020-06-12 2023-03-03 苏州九维电气制造有限公司 High-stability self-curing insulation protection packaging material and preparation method thereof
CN112608714A (en) * 2020-12-17 2021-04-06 成都硅宝新材料有限公司 Industrial heat-resistant silane modified polyether sealant and preparation method thereof
CN112980374B (en) * 2021-03-24 2022-12-30 杭州之江新材料有限公司 Two-component silane modified sealant and preparation method thereof

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